CN108558213A - Fluorescent glass ceramic material, method for manufacturing same, and light emitting device including same - Google Patents

Fluorescent glass ceramic material, method for manufacturing same, and light emitting device including same Download PDF

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Publication number
CN108558213A
CN108558213A CN201810074684.8A CN201810074684A CN108558213A CN 108558213 A CN108558213 A CN 108558213A CN 201810074684 A CN201810074684 A CN 201810074684A CN 108558213 A CN108558213 A CN 108558213A
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weight
ceramic material
glass ceramic
fluorescent
fluorescent glass
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刘伟仁
张之辰
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Chung Yuan Christian University
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Chung Yuan Christian University
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0009Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02Use of particular materials as binders, particle coatings or suspension media therefor
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/06Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/006Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of microcrystallites, e.g. of optically or electrically active material
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    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/062Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/066Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
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    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/076Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
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    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00Compositions for glass with special properties
    • C03C4/12Compositions for glass with special properties for luminescent glass; for fluorescent glass
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/58Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
    • C09K11/582Chalcogenides
    • C09K11/584Chalcogenides with zinc or cadmium
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    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7774Aluminates
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50Wavelength conversion elements
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50Wavelength conversion elements
    • H01L33/501Wavelength conversion elements characterised by the materials, e.g. binder
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50Wavelength conversion elements
    • H01L33/501Wavelength conversion elements characterised by the materials, e.g. binder
    • H01L33/502Wavelength conversion materials
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/52Encapsulations
    • H01L33/56Materials, e.g. epoxy or silicone resin
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2214/00Nature of the non-vitreous component
    • C03C2214/16Microcrystallites, e.g. of optically or electrically active material

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  • Dispersion Chemistry (AREA)
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  • Luminescent Compositions (AREA)

Abstract

The invention provides a fluorescent glass ceramic material, a manufacturing method thereof and a light-emitting device comprising the same. The fluorescent glass ceramic material comprises a glass material and fluorescent powder, wherein the glass material comprises SiO2、Al2O3、Na2O、K2O, CaO and B2O3. The fluorescent glass ceramic material, the manufacturing method thereof and the light-emitting device comprising the fluorescent glass ceramic material can avoid the problems of deterioration and yellowing caused by the traditional packaging material, thereby improving the light-emitting efficiency of the light-emitting device.

Description

Fluorescent glass ceramic material, its manufacturing method and the light-emitting device including it
Technical field
The present invention relates to a kind of glass ceramic material, its manufacturing method and light-emitting devices, are related to a kind of fluorescent glass pottery especially Ceramic material, its manufacturing method and light-emitting device.
Background technology
Light emitting diode (light emitting diode, LED) is in addition to low power consuming, small, brightness is high, uses The advantages that long lifespan and one kind meeting environmental protection and energy-efficient green light source.In general, include the luminous dress of light emitting diode Set mainly with fluorescent powder and resin-bonded at encapsulating material be packaged, however the encapsulating material is under long-time use There is the problem of deterioration and yellow, and then reduces the luminous efficiency of light-emitting device.
Invention content
The present invention provides a kind of fluorescent glass ceramic material, its manufacturing method and the light-emitting device including it, can avoid passing Unite encapsulating material caused by deterioration and yellow the problem of, and then improve light-emitting device luminous efficiency.
The present invention proposes a kind of fluorescent glass ceramic material, including glass material and fluorescent powder.Glass material includes SiO2、Al2O3、Na2O、K2O, CaO and B2O3
In one embodiment of this invention, in above-mentioned fluorescent glass ceramic material, with glass material and fluorescent powder Total weight, glass material can be 90 weight % to 99 weight %, and fluorescent powder can be 1 weight % to 10 weight %.
In one embodiment of this invention, in above-mentioned fluorescent glass ceramic material, glass material may include 67.2 weights Measure the SiO of % to 82.1 weight %2, 6.5 weight % to 8 weight % Al2O3, 5.5 weight % to 6.7 weight % Na2O、 The K of 1.7 weight % to 2.1 weight %2O, the CaO and 8.4 weight % of 0.7 weight % to 0.9 weight % is to 10.3 weight %'s B2O3
In one embodiment of this invention, in above-mentioned fluorescent glass ceramic material, fluorescent powder may include (Y, Lu, Gd)3(Al,Ga)5O12:Ce3+、(Ca,Sr,Ba)2Si5N8:Eu2+、(Sr,Ca)AlSiN3:Eu2+、α-SiAlON:Eu2+、β- SiAlON:Eu2+、(Ca,Sr,Ba)2SiO4:Eu2+、(Ca,Sr,Ba)Si2O2N2:Eu2+Or K2(Si,Ti)F6:Mn4+
The present invention proposes a kind of manufacturing method of fluorescent glass ceramic material, includes the following steps.To glass material with it is glimmering Light powder carries out mixed processing, and to form mixture, wherein glass material includes SiO2、Al2O3、Na2O、K2O, CaO and B2O3.It is right Mixture is sintered.Cooling processing is carried out to the mixture after sintering processes, and obtains fluorescent glass ceramic material.
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, glass material Material may include 67.2 weight % to the SiO of 82.1 weight %2, 6.5 weight % to 8 weight % Al2O3, 5.5 weight % to 6.7 The Na of weight %2O, the K of 1.7 weight % to 2.1 weight %2O, the CaO and 8.4 weight % of 0.7 weight % to 0.9 weight % be extremely The B of 10.3 weight %2O3
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, fluorescent powder It may include (Y, Lu, Gd)3(Al,Ga)5O12:Ce3+、(Ca,Sr,Ba)2Si5N8:Eu2+、(Sr,Ca)AlSiN3:Eu2+、α- SiAlON:Eu2+、β-SiAlON:Eu2+、(Ca,Sr,Ba)2SiO4:Eu2+、(Ca,Sr,Ba)Si2O2N2:Eu2+Or K2(Si,Ti) F6:Mn4+
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, mixing In processing, with the total weight of glass material and fluorescent powder, e.g. by 90 weight % to the glass material and 1 of 99 weight % The fluorescent powder of weight % to 10 weight % mixes.
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, burnt Sintering temperature when knot processing can be 800 DEG C~1200 DEG C.
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, at cooling Reason is, for example, to use Temperature fall method.
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, can more it wrap It includes after mixed processing, and before sintering processes, mixture is carried using carrying tablet.
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, carrying tablet E.g. quartzy cotton piece.
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, can more it wrap It includes after cooling processing, fluorescent glass ceramic material is made to be detached with carrying tablet.
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, can more it wrap It includes and fluorescent glass ceramic material is cut into sheet.
Described in one embodiment of the invention, in the manufacturing method of above-mentioned fluorescent glass ceramic material, sheet Fluorescent glass ceramic material thickness can be 0.01 millimeter (mm) to 10 millimeters.
The present invention proposes a kind of light-emitting device, including light emitting diode and above-mentioned fluorescent glass ceramic material.Fluorescence glass Glass ceramic material covers light emitting diode.
Described in one embodiment of the invention, in above-mentioned light-emitting device, the wavelength of light emitting diode can be received for 254 Rice (nm) is to 480 nanometers.
Described in one embodiment of the invention, in above-mentioned light-emitting device, the shape of fluorescent glass ceramic material can For sheet.
Based on above-mentioned, in fluorescent glass ceramic material proposed by the invention and its manufacturing method, due to above-mentioned fluorescence Glass ceramic material includes glass material and fluorescent powder, and glass material includes SiO2、Al2O3、Na2O、K2O, CaO and B2O3, because This can have high thermal stability, high-cooling property, high light transmittance, and then be avoided that the deterioration caused by conventional encapsulant and Huang The problem of change.Further, since light-emitting device proposed by the invention is luminous to cover by above-mentioned fluorescent glass ceramic material Diode, therefore can have preferable luminous efficiency.
To make the foregoing features and advantages of the present invention clearer and more comprehensible, special embodiment below, and coordinate shown attached drawing It is described in detail below.
Description of the drawings
Fig. 1 is the schematic diagram of the fluorescent glass ceramic material of one embodiment of the invention.
Fig. 2 is the flow chart of the manufacturing method of the fluorescent glass ceramic material of one embodiment of the invention.
Fig. 3 is the schematic diagram of the light-emitting device of one embodiment of the invention.
Fig. 4 is the fluorescence spectrum of the fluorescent glass ceramic material obtained by experimental example 1.
Fig. 5 is the alternating temperature spectrum of the fluorescent glass ceramic material obtained by experimental example 1.
Fig. 6 is the fluorescent glass ceramic material and general business fluorescent powder YAG obtained by experimental example 1:Ce3+Progress Alternating temperature spectrum after standardization.
Fig. 7 is the constant current electroexcitation spectrum of the light-emitting device obtained by experimental example 2 to 4.
Fig. 8 is the constant current electroexcitation spectrum of the light-emitting device obtained by experimental example 5 to 7.
Fig. 9 is the time-dependent current electroexcitation spectrum of the light-emitting device obtained by experimental example 3.
Figure 10 is the time-dependent current electroexcitation spectrum of the light-emitting device obtained by experimental example 6.
Reference sign:
100:Fluorescent glass ceramic material
110:Glass material
120:Fluorescent powder
200:Light-emitting device
210:Light emitting diode
S100、S110、S120、S130、S140、S150:Step
Specific implementation mode
Fig. 1 is the schematic diagram of the fluorescent glass ceramic material of one embodiment of the invention.
Fig. 1 is please referred to, fluorescent glass ceramic material 100 includes glass material 110 and fluorescent powder 120.Fluorescent glass is made pottery The shape of ceramic material 100 can be sheet.With the total weight of glass material 110 and fluorescent powder 120, glass material 110 can be 90 weight % to 99 weight %, and fluorescent powder 120 can be 1 weight % to 10 weight %.
Glass material 110 includes SiO2、Al2O3、Na2O、K2O, CaO and B2O3(it can also use SiO2-Al2O3-Na2O-K2O- CaO-B2O3To indicate).Glass material may include 67.2 weight % to the SiO of 82.1 weight %2, 6.5 weight % to 8 weight % Al2O3, 5.5 weight % to 6.7 weight % Na2O, the K of 1.7 weight % to 2.1 weight %2O, 0.7 weight % to 0.9 weight Measure the B of the CaO and 8.4 weight % to 10.3 weight % of %2O3
In addition, fluorescent powder 120 may include (Y, Lu, Gd)3(Al,Ga)5O12:Ce3+、(Ca,Sr,Ba)2Si5N8:Eu2+、(Sr, Ca)AlSiN3:Eu2+、α-SiAlON:Eu2+、β-SiAlON:Eu2+、(Ca,Sr,Ba)2SiO4:Eu2+、(Ca,Sr,Ba)Si2O2N2: Eu2+Or K2(Si,Ti)F6:Mn4+
Based on above-described embodiment it is found that since fluorescent glass ceramic material 100 includes glass material 110 and fluorescent powder 120, And glass material 110 includes SiO2、Al2O3、Na2O、K2O, CaO and B2O3, therefore can have high thermal stability, high-cooling property, height Translucency, and then the problem of be avoided that the deterioration caused by conventional encapsulant and yellow.In addition, fluorescent glass ceramic material 100 can apply in the encapsulation of the light-emitting devices such as LED, and have good optical appearance after optic test, so that Light-emitting device with fluorescent glass ceramic material 100 can be applied in high power illumination and all kinds of screen displays.
Fig. 2 is the flow chart of the manufacturing method of the fluorescent glass ceramic material of one embodiment of the invention.
The manufacturing method of the fluorescent glass ceramic material of the present embodiment is for making the fluorescent glass ceramic material of Fig. 1 100 illustrate, but the present invention is not limited thereto.The detailed description of each component of fluorescent glass ceramic material 100 can be joined According to the explanation of above-described embodiment, it is not repeated to illustrate in this.
Fig. 1 and Fig. 2 are please referred to, step S100 is carried out, mixed processing is carried out to glass material 110 and fluorescent powder 120, with shape Resulting mixture, wherein glass material 110 include SiO2、Al2O3、Na2O、K2O, CaO and B2O3.For example, in mixed processing In, it, can be by the glass material of 90 weight % to 99 weight % and 1 weight % extremely with the total weight of glass material and fluorescent powder The fluorescent powder of 10 weight % mixes.
Glass material 110 in the mixture may include 67.2 weight % to the SiO of 82.1 weight %2, 6.5 weight % extremely The Al of 8 weight %2O3, 5.5 weight % to 6.7 weight % Na2O, the K of 1.7 weight % to 2.1 weight %2O, 0.7 weight % To the B of the CaO and 8.4 weight % to 10.3 weight % of 0.9 weight %2O3
In addition, fluorescent powder 120 in the mixture may include (Y, Lu, Gd)3(Al,Ga)5O12:Ce3+、(Ca,Sr,Ba)2Si5N8:Eu2+、(Sr,Ca)AlSiN3:Eu2+、α-SiAlON:Eu2+、β-SiAlON:Eu2+、(Ca,Sr,Ba)2SiO4:Eu2+、 (Ca,Sr,Ba)Si2O2N2:Eu2+Or K2(Si,Ti)F6:Mn4+
Step S110 is optionally carried out, mixture is carried using carrying tablet.Carrying tablet is, for example, quartzy cotton piece.
Step S120 is carried out, mixture is sintered.Sintering temperature when being sintered can be 800 DEG C~ 1200 DEG C, such as 900 DEG C.For example, sintering processes may include the following steps.First, mixture is placed in high temperature furnace, then existed It is heated up with 5 DEG C of heating rate per minute in air atmosphere, and temperature is held respectively when temperature rise to 300 DEG C and 600 DEG C 30 minutes.Finally, when being warming up to 900 DEG C with 5 DEG C of heating rate per minute, temperature is held 4 hours.
Step S130 is carried out, cooling processing is carried out to the mixture after sintering processes, and obtains fluorescent glass ceramics material Material 100.Cooling processing is, for example, that the temperature of the mixture after sintering processes is down to room temperature using Temperature fall method.It is real herein It applies in example, the fluorescent glass ceramic material 100 obtained can be bulk.
Step S140 is optionally carried out, fluorescent glass ceramic material 100 is made to be detached with carrying tablet.
Step S150 is optionally carried out, fluorescent glass ceramic material 100 is cut into sheet.The wherein fluorescence of sheet The thickness of glass ceramic material is, for example, 0.01mm to 10mm.
Based on above-described embodiment it is found that the fluorescent glass produced by the manufacturing method of fluorescent glass ceramic material 100 is made pottery Ceramic material 100 can have high thermal stability, high-cooling property, high light transmittance, and then be avoided that bad caused by conventional encapsulant The problem of change and yellow.In addition, fluorescent glass ceramic material 100 can apply in the encapsulation of the light-emitting devices such as LED, and pass through There is good optical appearance, so that the light-emitting device with fluorescent glass ceramic material 100 can be applied after optic test In high power illumination and all kinds of screen displays.
Fig. 3 is the schematic diagram of the light-emitting device of one embodiment of the invention.
Hereinafter, illustrating the embodiment that the fluorescent glass ceramic material 100 of Fig. 1 is applied to light-emitting device by Fig. 3.This Outside, identical element and is not repeated to illustrate with identical symbolic indication in Fig. 3 and Fig. 1.
Fig. 3 is please referred to, light-emitting device 200 includes light emitting diode 210 and fluorescent glass ceramic material 100, wherein glimmering Light glass ceramic material 100 covers light emitting diode 210.The wavelength of light emitting diode can be 254nm to 480nm.
Based on above-described embodiment it is found that since light-emitting device 200 uses fluorescent glass ceramic material 100 to be used as package material The problem of expecting, therefore can avoid the deterioration and yellow caused by conventional encapsulant, and there is good optical appearance, thus It can be applicable to high power illumination and all kinds of screen displays.
Hereinafter, by experimental example come the effect of confirming above-described embodiment, but the range Bing Bu Authority of the present invention are limited in following Hold.
<Experimental example>
<Experimental example 1 to the fluorescent glass ceramic material of experimental example 7 preparation method>
First, according to the type and weight of glass material shown in the following table 1 and fluorescent powder, to glass material and fluorescent powder into Row mixed processing, to form mixture.Glass material uses SiO2-Al2O3-Na2O-K2O-CaO-B2O3, wherein glass material packet Include the SiO of 74.64 weight %2, 7.27 weight % Al2O3, 6.06 weight % Na2O, the K of 1.91 weight %2O, 0.79 weight Measure the B of the CaO and 9.32 weight % of %2O3
Table 1
Then, experimental example 1 is carried respectively to the mixture of experimental example 7 using quartzy cotton piece.Then, mixture is placed in high Warm stove is sintered, and wherein sintering processes include the following steps.With 5 DEG C per minute of heating rate liter in air atmosphere Temperature, and when temperature rise to 300 DEG C and 600 DEG C, temperature is held respectively 30 minutes.Finally, with 5 DEG C of heating rate per minute When being warming up to 900 DEG C, temperature is held 4 hours.
Later, the mixture after sintering processes of experimental example 1 to experimental example 7 is carried out at cooling with Temperature fall method Reason, makes temperature be reduced to room temperature, and forms block-like fluorescent glass ceramic material.Followed by, make quartzy cotton piece and block-like fluorescence Glass ceramic material detaches.Furthermore block-like fluorescent glass ceramic material is cut into sheet, wherein experimental example 1 to experimental example 7 The thickness of obtained fluorescent glass potsherd is as shown in table 1.
<Spectrofluorimetry>
Fig. 4 is the fluorescence spectrum of the fluorescent glass ceramic material obtained by experimental example 1.
Spectrofluorimetry is carried out to the fluorescent glass ceramic material obtained by experimental example 1, the results are shown in Figure 4, experiment The fluorescent glass ceramic material of example 1 and general business fluorescent powder YAG:Ce3+Fluorescence spectrum it is roughly the same.
<Alternating temperature spectrum analysis>
Fig. 5 is the alternating temperature spectrum of the fluorescent glass ceramic material obtained by experimental example 1.Fig. 6 is obtained by experimental example 1 Fluorescent glass ceramic material and general business fluorescent powder YAG:Ce3+Be standardized after alternating temperature spectrum.
To the fluorescent glass potsherd and fluorescent powder YAG obtained by experimental example 1:Ce3+Alternating temperature spectrum analysis is carried out respectively.
According to Fig. 5's as a result, temperature change is to wavelength value of the fluorescent glass potsherd at wave crest obtained by experimental example 1 Influence is very small, so illustrating that the fluorescent glass potsherd has very high thermal stability.
Fig. 6 is the fluorescent glass potsherd and general business fluorescent powder YAG obtained by experimental example 1:Ce3+Carry out standard Alternating temperature spectrum after change.According to Fig. 6's as a result, when temperature is identical, the standardization of the fluorescent glass potsherd of experimental example 1 shines Intensity is larger, so illustrating that the fluorescent glass potsherd has high-cooling property.
<Experimental example 2 to the light-emitting device of experimental example 7 preparation method>
The fluorescent glass potsherd of above-mentioned experimental example 2 to 7 is covered each by same light emitting diode, to be fabricated to six A light-emitting device, and the wavelength for the light that wherein light emitting diode is sent out is 450nm to 460nm.
<Constant current electroexcitation spectrum analysis>
Fig. 7 is the constant current electroexcitation spectrum of the light-emitting device obtained by experimental example 2 to 4.Fig. 8 is 5 to 7 institute of experimental example The constant current electroexcitation spectrum of light-emitting device obtained.
Carry out constant current electroexcitation spectrum analysis, result such as Fig. 7 respectively to the light-emitting device comprising experimental example 2 to 4 It is shown.In addition, the light-emitting device of experimental example 5 to 7 to be carried out to constant current electroexcitation spectrum analysis respectively, the results are shown in Figure 8. Wherein, in Fig. 7 and Fig. 8, left side is the spectrum of light emitting diode, and right side is the spectrum of fluorescent glass potsherd.In addition, root According to Fig. 7 and Fig. 8 it is found that when the thickness of fluorescent glass potsherd increases, the luminous intensity of light emitting diode reduces, and fluorescence glass The luminous intensity of glass potsherd is relatively high, so light-emitting device can be changed by being adjusted by the thickness of fluorescent glass potsherd Luminescent color.
<Cie color is analyzed>
International Commission on Illumination (CIE) colorimetric analysis, result such as 2 institute of table are carried out to the light-emitting device of experimental example 2 to 7 Show.
Table 2
According to table 2 it is found that hair can be changed by being adjusted by the thickness of the fluorescent glass potsherd obtained by experimental example 2 to 7 The luminescent color of electro-optical device.
<Time-dependent current electroexcitation spectrum analysis>
Fig. 9 is the time-dependent current electroexcitation spectrum of the light-emitting device obtained by experimental example 3.Figure 10 is obtained by experimental example 6 Light-emitting device time-dependent current electroexcitation spectrum.
Time-dependent current electroexcitation spectrum analysis, result point are carried out to the light-emitting device obtained by experimental example 3 and experimental example 6 Not not as shown in Figures 9 and 10.In Fig. 9 and Figure 10, left side is the spectrum of light emitting diode, and right side is fluorescent glass ceramics The spectrum of piece.In addition, according to the result of Fig. 9 and Figure 10 it is found that curent change is to the fluorescence obtained by experimental example 3 and experimental example 6 Glass ceramics piece and wavelength value influence of the light emitting diode at wave crest are very small, so illustrating curent change to experimental example 3 With the influence very little of the luminescent color of the light-emitting device of experimental example 6.
<Luminous efficiency is tested>
Luminous efficiency test is carried out to the light-emitting device obtained by experimental example 2 to 7, the results are shown in Table 3.
Table 3
According to table 3 it is found that the light-emitting device obtained by experimental example 2 to 7 has very high luminous efficiency.
In conclusion in the fluorescent glass ceramic material of above-described embodiment, its manufacturing method and including its light-emitting device In, since the glass material in fluorescent glass ceramic material has specific composition, it can avoid conventional encapsulant and made At deterioration and yellow the problem of, and then improve light-emitting device luminous efficiency.
Although the present invention has been disclosed by way of example above, it is not intended to limit the present invention., any people in the art Member, without departing from the spirit and scope of the present invention, when can make some changes and embellishment, therefore protection scope of the present invention is when regarding Subject to those as defined in claim.

Claims (18)

1. a kind of fluorescent glass ceramic material, which is characterized in that including:
Glass material, including SiO2、Al2O3、Na2O、K2O, CaO and B2O3;And
Fluorescent powder.
2. fluorescent glass ceramic material according to claim 1, which is characterized in that with the glass material and described glimmering The total weight of light powder, the glass material is 90 weight % to 99 weight %, and the fluorescent powder is 1 weight % to 10 weights Measure %.
3. fluorescent glass ceramic material according to claim 1, which is characterized in that the glass material includes 67.2 weights Measure the SiO of % to 82.1 weight %2, 6.5 weight % to 8 weight % Al2O3, 5.5 weight % to 6.7 weight % Na2O、 The K of 1.7 weight % to 2.1 weight %2O, the CaO and 8.4 weight % of 0.7 weight % to 0.9 weight % is to 10.3 weight %'s B2O3
4. fluorescent glass ceramic material according to claim 1, which is characterized in that the fluorescent powder includes (Y, Lu, Gd)3 (Al,Ga)5O12:Ce3+、(Ca,Sr,Ba)2Si5N8:Eu2+、(Sr,Ca)AlSiN3:Eu2+、α-SiAlON:Eu2+、β-SiAlON: Eu2+、(Ca,Sr,Ba)2SiO4:Eu2+、(Ca,Sr,Ba)Si2O2N2:Eu2+Or K2(Si,Ti)F6:Mn4+
5. a kind of manufacturing method of fluorescent glass ceramic material, which is characterized in that including:
Mixed processing is carried out to glass material and fluorescent powder, to form mixture, wherein the glass material includes SiO2、 Al2O3、Na2O、K2O, CaO and B2O3
The mixture is sintered;And
Cooling processing is carried out to the mixture after sintering processes, and obtains fluorescent glass ceramic material.
6. the manufacturing method of fluorescent glass ceramic material according to claim 5, which is characterized in that the glass material packet 67.2 weight % are included to the SiO of 82.1 weight %2, 6.5 weight % to 8 weight % Al2O3, 5.5 weight % to 6.7 weight % Na2O, the K of 1.7 weight % to 2.1 weight %2O, the CaO and 8.4 weight % to 10.3 weights of 0.7 weight % to 0.9 weight % Measure the B of %2O3
7. the manufacturing method of fluorescent glass ceramic material according to claim 5, which is characterized in that the fluorescent powder includes (Y,Lu,Gd)3(Al,Ga)5O12:Ce3+、(Ca,Sr,Ba)2Si5N8:Eu2+、(Sr,Ca)AlSiN3:Eu2+、α-SiAlON:Eu2+、 β-SiAlON:Eu2+、(Ca,Sr,Ba)2SiO4:Eu2+、(Ca,Sr,Ba)Si2O2N2:Eu2+、K2(Si,Ti)F6:Mn4+
8. the manufacturing method of fluorescent glass ceramic material according to claim 5, which is characterized in that in the mixed processing In, with the total weight of the glass material and the fluorescent powder, by 90 weight % to the glass material of 99 weight % It is mixed with the fluorescent powder of 1 weight % to 10 weight %.
9. the manufacturing method of fluorescent glass ceramic material according to claim 5, which is characterized in that carry out at the sintering Sintering temperature when reason is 800 DEG C~1200 DEG C.
10. the manufacturing method of fluorescent glass ceramic material according to claim 5, which is characterized in that the cooling processing Including using Temperature fall method.
11. the manufacturing method of fluorescent glass ceramic material according to claim 5, which is characterized in that further include described After mixed processing, and before the sintering processes, the mixture is carried using carrying tablet.
12. the manufacturing method of fluorescent glass ceramic material according to claim 11, which is characterized in that the carrying tablet packet Include quartzy cotton piece.
13. the manufacturing method of fluorescent glass ceramic material according to claim 11, which is characterized in that further include described After cooling processing, the fluorescent glass ceramic material is made to be detached with the carrying tablet.
14. the manufacturing method of fluorescent glass ceramic material according to claim 5, which is characterized in that further including will be described Fluorescent glass ceramic material is cut into sheet.
15. the manufacturing method of fluorescent glass ceramic material according to claim 14, which is characterized in that sheet it is described glimmering Light glass ceramic material thickness is 0.01 millimeter to 10 millimeters.
16. a kind of light-emitting device, which is characterized in that including:
Light emitting diode;And
Fluorescent glass ceramic material according to claim 1, covers the light emitting diode.
17. light-emitting device according to claim 16, which is characterized in that the wavelength of the light emitting diode is 254 nanometers To 480 nanometers.
18. light-emitting device according to claim 16, which is characterized in that the shape of the fluorescent glass ceramic material includes Sheet.
CN201810074684.8A 2017-10-05 2018-01-25 Fluorescent glass ceramic material, method for manufacturing same, and light emitting device including same Pending CN108558213A (en)

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Application publication date: 20180921